Education in analytical chemistry. Comments - ACS Publications

Lin Huang , Shuyan Qiu , Neissa M. Pinzon , Li-ta Lien , Lu-Kwang Ju. Environmental Engineering Science 2008 25 (3), 439-450 ...
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-A View From Industry

“New Horizons in Education,” which appeared in the February 1966 issue of ANALYTICAL CHEMISTRY, evoked an immediate interest from the readers of the journal. It appears that the subject of education in analytical chemistry, viewed on a national scale, has remained dormant €or all too long. The February article was drawn entirely from the academic cominunity; the present article contains the ideas of analytical chemists long familiar with the problems of industry. THE FEATURE ARTICLE

Even before publication of the February article, i t became apparent to the Editors that the opinions of some outstanding analytical chemists in industry should be sampled, in order to place the problems of education in better perspective. Each of the contributors to the present article was allowed complete freedoni to expound on the problems as he sees them, and to comment on the views expressed in “New Horizons in Education” [ANAL. CHEM.38, 35A (February 1966>]. Following are their individual comments: VOL. 38, NO. 13, DECEMBER 1966

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REPBRT FOR ANALYTICAL CHEMISTS

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It is difficult for the analytical chemist in industry t o visualize a “second rate status” for his discipline when he plays such a vital role in almost every activity of his company. At the reseurch phase, he is usually the one to first determine that a certain product was made. H e usually is also involved in determining the yields obtained at the various conditionu, the impurities present, the stability and solubilities of material, and physical constants. At the research phase, the analytical chemist develops new methods of analysis important to the technology of his company. H e also investigates the new developments of others in the field t o see if, and how, they can be applied to his company’s problems. At the development phase of chemical operations, the analytical chemist develops control analyticd methods and 30A

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helps gain further knowledge ‘of the system under scaled-up conditions. At the production phase, processes are monitored analytically to ensure optimized operation a t each step and also the final product is monitored for specification purposes. Almost all purchased chemical materials are monitored analytically. Any trouble (yield loss, catalyst failure, explosion, fire, corrosion, quality decrease) is immediately investigated analytically. I n the sales portion of the chemical business, competitor products must be analyzed as an “intelligence” function. ,4190, customer complaints must be handled via analysis of any offending shipments of material, and customer good-will is established and maintained by supplying t o customers analyses or analytical methods involving the products being sold to them. I n the legal part of the chemical business, analysis establishes or refutes alleged

patent infringement; also, analysis establishes or refutes a company’s liability for damage to life and/or property allegedly caused by a product. Into the legal area also falls the large amount of analytical activity involved in obtaining Food & Drug, Department of Agriculture, or other Government clearances to use certain materials. Even m a n agement decisions often involve analysis. Ventures are undertaken or located based on analyses of mineral deposits; analysis of local water can best locate certain plants ; processes are purchased based on product analysis ; major projects are undertaken or dropped as a result of analysis of competitive products. From the above summary, it should be quite apparent that the analytical chemist plays a major role in the industrial scheme of things. It should also be apparent that the work requested is not just

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iwer is general mantical Instruments Dim vision of Teledyne, Inc. located in Pasadena, Calif. He received A B . PAN-pH and M.A. degrees in chemistry from INDICATOR PAPERS Stanford University and a Ph. D. from An i m p r o v e d m e t h o d for pH determination. MIT. Dr. Gardiner’s former indusS i m p l e t o u s e . P r o v i d e s p r e c i s e result. trial associations were with Bros., Firestone Tire and 25 d i f f e r e n t pH values easily Company, Continental Can Co r e a d in t h e 0.1 t o 14 pH range and Bell and ~ o w e ~ ~ - C o n s o l i d a ~ e ~ PAN.pH I n d i c a t o r S t r i p s p r o v i d e clear.cut visual determination of color values i n the Electrodyna m ics. His membersh i ps 0.1 t o 1 4 pH range. From pH 0.1 t o 10, values include Sigma Xi, Phi can b e accurately determined t o within one half of a pH unit, and i n the pH range from Alpha Chi Sigma, and

routine work but much of i t is difficult, challenging, and important, and that i t requires drive, ability, If training, and responsibility. analysis were to disappear in industry, almost every phase of industrial activity vould be severely hampered, if not stopped completely. Although the “status” of the analytical chemist in industry is as high as that of any other technical man, just like any other man, the analyst must earn his status. The reason t h a t the deserving analyst ranks high is that he is needed, and in satisfying company needs, the analyst is appreciated. The above discussion should make it apparent that the industrial demand for analytical chemists is high. However, the supply of graduates interested in analytical chemistry is low, especially for those with advanced degrees. The demand is so high that we in industry often employ “near analytical chemists”

and orient them accordingly to make what we need. A “near analytical chemist” is a physical, inorganic, or organic major svhose thesis work was heavy in analytical type syork such as structure proofs, spectroscopy, instrumentation, and the like. With the high demand, we find these men difficult to hold once we have trained them. They easily find other jobs and a t premium salaries. Thus, \ye in industry find ourselves as one of the prime trainers of men needed by the field, and must supplement or complement the schools. I would approximate that about 50% of the practicing analytical chemists with advanced degrees did not get their degrees in analytical chemistry. As a practitioner of analytical chemistry, I have dealt with many graduates from many schools in all phases of chemical activity: synthesis, engineering, physical as well as analytical. From thwe men I

10 t o 14, pH determinations are accurate to w i t h i n 1 pH unit. E i n d i c a t o r colors used for each comparison PAN.pH differs from former methods i n t h a t 8 different and separate indicator COlOrS are used f o r each strip, i n a sequence which makes i t simple t o match pH values against a master chart. Greater accuracy When d i p p e d i n t o a s o l u t i o n t o b e t e s t e d , the color change is read by means of changes i n shade o i more than one indicator Color. This serves t o increase accuracy by providi n g the scientist w i t h more than a single p o i n t of comparison. How PAN.pH d i f f e r s Instead of mixed dye coiors, PAN-pH papers use 8 individual single coiors as indicators, a l l of which are different. The bottom Color changes a t pH 0.1. Other color changes occur i n 0.5 pH intervals. The used indicator strip, after immersion i n the test solution, allows an easy comparison o i a l l 8 colors t o a corresponding 8.coIor master chart. Availability S&S PAN-pH indicator papers are available i n boxes containing 200 strips. Each box i n cludes detailed instructions and a master color chart. Box is a sturdy fold-back type w i t h a flip.top, f o r easy access t o strips, which are approximately 34:S“ long and 5/16” wide. Another S&S specialty This new pH indicator method was developed i n cooperation with Riedel.de Haen AG i n Seeize, Western Germany, and is marketed i n t h e U n i t e d S t a t e s b y Carl S c h l e i c h e r & Schueii Co.

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analytical chemistry should be physical principles. These princitaught. Having read the Report ples are relatively easy to teach for Analytical Chemists in the Febsince they follow a logical order; ruary 1966 issue of ANALYTICAL they are factual, and they are well CHEMISTRY ccncerning “New Horidescribed in textbooks. The funzons in Education,” I can find damental analytical principles are agreement with all comments to more difficult t o teach because some degree. It is axiomatic t h a t they are less factual and more philthe teaching of analytical chemistry osophical; they do follow a n order, include fundamental principles. but is not a fixed mathematical These principles form a foundation order. They are well described in on which the student can build any texts but possibly not all in one sort of future according to the dicplace. The analytical pattern of tates of his abilities, aptitudes, inthinking is very difficult to teach terests, his job, and the times. This because i t is a frame of mind. The foundation remains ralid over the practicing analyst is aware of this years while the “architecture” of the frame of mind because it is part of superstructure may change with the his make-up through practicing the fashions of the times. These are field. Some competent academic fads and fashions in chemical analmen in analysis have never pracysis as there are in all fields. ticed the field in industry and can However, when I look a t ‘,fundahare understandable difficulty conmental principles” in regard to veying this aspect to students. It analysis, I see more than just fundaactually may be very wise for all mental physical principles. The teachers of analysis to take periodic analytical chemist must also be summer jobs in industry to maininbred with fundamental analytical tain a perspectire and also t o gain principles and an ihalytical pattern much factual information of which of thinking. These fundamental they were not aware. I n fact, such analytical principles concern theman exchange can be mutually adselves with a constant awareness vantageous. Industry is also a of: (1) accuracy and precision; good source for good ideas for re(2) sources of error; (3) the use of search programs. Analysis is a n several approaches to firm up a applied science and I feel i t would conclusion (confirmation) ; (4) sigbe difficult t o teach an applied scinificance of data. ence without having applied it. The analytical pattern of thinkI wish now to dwell on the idea of ing is what orients the student to“Big Science” since i t shuns the ward the application of the physical idea of the applied. The current principle. Analytical chemistry is fad of “Big Science” is one of the an applied science and we should be pressures on analytical chemistry. sure that the student is aware of Many teachers of analytical chemthis. The student’s “analytical” inistry in trying to meet the challenge doctrination should imprint him of ‘[Big Science” may go too far towith a sort of template that he autoward accenting only the basic physmatically will apply to all fundaical principle. These men may no mental principles and problems that longer be teaching analytical chemhe will encounter: what can I do istry. I have already discussed this with this approach, accuracy and above. The “Big Science” fad, precision, how conclusive is my rehowever, is a further threat to good sult, do I require more evidence, is analytical chemistry. Being heavy i t fast enough to be useful, what inwith theory, “Big Science” leans toterferences might be there. This acward the analytical approaches cent on the applied aspect of physibased on deep physical theory. cal theory and the value of the data This leads to ignoring some simare the essence of the analytical ple, very useful analytical apchemist and differentiate him from proaches, especially those based on the physicist and physical chemist chemical chemistry. It suffices t o who accent the physical principle say that the chemical properties of per se. chemical materials are very characThe educator in analytical chemteristic, as characteristic as any opistry can readily concentrate on the tical, electrical, thermal, magnetic, teaching of solely fundamental or other physical property, and

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hence make excellent “handles” for analysis. I n practice one finds that the chemical and physical methods I are both used with the job to be accomplished dictating the approaches used. Just like the power tools in carpentry have not displaced the I older hand tools, so the newer analytical approaches have not replaced the old. The analytical “tool kit” has just gotten bigger and bigger. Still another problem which has been introduced by the emphasis on “Big Science” also has to do with its emphasis on theory. With the accent on deep theory, too often experimentation is subordinated. This is critical in all chemical disciplines because theory must be proven. This is especially critical for analysis since analytical chemists gather data and this can be done only by experiment. With the current mood then, we see with greater frequency analytical workers coming out of the schools heavy with theory and mathematics. This is not bad a t all, but they often have too low a desire or understanding for BRUSH and for experimental work. Manual deULTRA-SONIC Washing tails become trivial. Yet, as all of all laboratory glassware, who have done analysis know all missile and outer space components. .used too well, attention t o detail is rewherever the ULTIMATE quired for good data. The most exin cleaning is ESSEYTIAL pensive analytical or physical in-where &y thing less would strument can be valueless if the be too EXPENSIVE 1 sample was incorrectly weighed, allowed to spatter on ashing or s o h tion, if the material was improperly compIeteIysampled, of if the solution was difreelyluted t o the mark while hot. I n analysis, the final result is only good if each step is well executed. without film or A good analyst must be indoctriresidue even in nated to run experiments and he be inbred with the discipline, COLD WATER! must manual and mental, that goes into the gathering of good data. People thinking, rely on his work-good although very important, is not enough. I am not saying in this discussion that we need more experimental work in our curricula and less theory, not in the least. The student should be taught all the basic theory but in the student’s existing laboratory work, the importance of experiment and good technique should be driven home. I can summarize by stating that analytical chemists in the field are highly regarded and in great de-

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mand. They have “status” and all the recognition, material and otherwise, that goes with it, as long as they can do a good job. The field is full of challenges for men of all levels, B.S.through Ph.D., with the man making the job. The work is exciting with each job a chemical “detective” story. As long as this need exists, there will be pressure on the schools to produce more analytical chemists. It is well for the schools to keep in mind that an analytical chemist must get answers, and these must be good answers. To do this he must have complete command of the field; the basic theories of chemistry and physics guide him to the best approaches chemical or physical to be used for the job a t hand; experimentation with good technique gives him the data he needs t o accomplish his goals.

E. C. DUNLOP The chemical industry is interested in analytical chemistry because i t is essential to its good performance. Analytical chemists provide the information that controls manufacturing processes as wall as the techniques for characterization of new materials from research laboratories. Because it is necessary to have competent personnel, we are concerned about the education and professional stature of analytical chemists. An analytical chemist in industry is as difficult t o define as his colleague in the academic field. I think we need to be more precise than Professor Reilley ( 1 ) who defines analytical chemistry as “what analytical chemists do.” Rather, I would describe analytical chemistry as that part of the science concerned with qualitative and quantitative measurements. These measurements relate to elemental composition, structure, and physical properties, and distinguish the analytical chemist from the chemist who makes chemicals. Obviously this is a broad classification and must be brought into focus for each group concerned. For example, some industrial companies deal only with metals and alloys whereas others manufacture only organic chemicals. Analytical chemistry is experiComments of

REPORl encing explosive growth; and, 8: Professor Reilley said, "These BII exciting times of change in ou science." Years ago some applica. tions of analytical chemistry re quired only "cook book" type ex. perimente. This idea may stil exist but it is only the viewpoint 0: the ill-informed. halytical &em. ists muat devise procedures anc techniques to handle the most com. plex mixturea and to covw b d ranges of concentration. Only witt ingenuity and broad scientific edw cation can they accomplish theii objectives. Today's industrial ana. lytical group may include scientistr trained in several fields such as enjneering, mathematics, phyaws: md chemistry. To adequatelystaff ;he modem laboratory and to make efficient use of available equipment require the cooperative efforts of electmnic engineers or physieiste ta see that equipment performs, chemists to plan experiments and interpret the results, and mathematicians to devise program8 foE computer processing of data. & practice the industrial analytical organization is made up of p e r m e l who may perform as individuala or as a team and it is necessary that they be highly skilled in the areas in which they work. Analytical chemistry has become 80 broad in scope that we cannot expect graduate analytical chemists, much less undergraduate chemktry majors, to be expert in all its facets, e.g., solution chemistry, electrochemistry, spectroscopy (abrptiou and ermb aon) , polymer characterization, physical property mewremente, xray diffraction, microffiopy,sepamtions, radiochemistry, etc. Instead, ve hope the analytical chemist in educated" to make we of basic hemical principles and apply them 1 a quantitative mamm. This ia rue for both industrial and am-emic analytical chemists. As mentioned hy F'rofeasor Reinmuth and others, the career of an analytical chemist spans many Years during which new methods and techniques will be developed. Also some of the current methods may become leee important so personnel must be capable and m'lling to make changes and became 88 expert in a new field as they wem in their previous areas. Thus we

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would like a strong analytical chemistry division in every college to teach the basic principles of chemical equilibria, separations, electrochemistry, and the various types of spectroscopy so that the student will have knowledge about the significance of experimental data, training to develop practical experimental conditions in order to obtain meaningful data, and satisfaction experienced through obtaining quantitative results. If this basic background is obtained in the undergraduate curriculum, it should be possible for the analytical chemist to specialize and make highly satisfactory contributions in several different techniques throughout his career. Industrial analytical chemists are in the position that they must work with techniques that are applicable t o the products of their company while the academic professor can control his program and work in the area of electrochemistry, spectroscopy or whatever he chooses throughout his career. Thus if, after some years, it is necessary to change fields, the analytical chemist in industry must have continued to educate himself by constant reading of literature so that he is quickly able to grasp a new technique. It is often a practice in industry to encourage staff members t o take special courses to help them start in a new field or gain special information. These courses are highly valuable and, as Professor Reinniuth ( 2 ) stated in his discussion, “his viewpoint” gives the analytical chemist ability to make use quickly of information obtained from specialized courses. While basic principles are extremely important, it is necessary in the education program to illustrate these with practical examples. Here the analytical chemist will encounter interesting problems that show how he can join forces with chemists in other fields who really need his contribution in order to make their work most useful. I do not think it is necessary to have a uniform analytical curriculum in all colleges and universities. It is only natural that individual professors in analytical chemistry like professors in other fields will emphasize their specialty and in this way certain schools will

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educate students to be experts in certain areas. Industries will be able to obtain spectroscopists from some schools, radiochemists from other schools, and so forth. The analytical chemist must have sufficent education in all fields of chemistry (organic, inorganic, bio-, physical and engineering) in order to apply modern chemistry and instrunlentation to problems so that his measurements are informative. I n my opinion the undergraduate chemist should have a good course in the freshman or sophomore year emphasizing quantitative measurements and covering basic principles of solution chemistry, separations, electrochemistry, and spectroscopy. I n the senior year there should be a specialized course related t o problem solving involving spectroscopic-structure techniques and separation-identification-measuring methods which takes advantage of the particular professor’s field of research. This course should be divided when possible between the various professors in analytical chemistry so that experience could be obtained from each. I feel this mould be stimulating to the student and could lead t o a career in analytical chemistry directly or through the graduate school. ( 1 ) Reillep, C. S.,ANAL.CHEM.38, 35 A

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ical chemists could be and are taught in other courses (in freshman general chemistry and in physical chemistry, particularly) , the objectives of these courses differ considerably from those of the analytical chemistry course. The course in analytical chemistry is still needed to teach a point of view, to teach the student what the analytical chemist does. It is quite true that many who have completed graduate work in analytical chemistry have worked on research problems Jvhich could almost equally well have been classified as physical chemistry problems. However, when vie talk to candidates for employment in analytical chemistry research, Tve find that the man \Tho has completed the requirements for a degree in analytical chemistry has an appreciation for the problems of the analytical chemist and an interest in such problems. On the contrary the physical chemistry graduate is often thoroughly indoctrinated with the idea that analytical chemistry is somehow a profession unworthy of his efforts. He often shows little appreciation for the problems of the analytical chemist and frequently shows a certain amount of disdain a t the thought of being asked to consider employment in that field. At the same time we find that our physical chemist colleagues are eager t o talk with candidates trained as analytical chemists and that they are not infrequently able to inbue them with the idea that work in their field is somehow superior t o that of the analytical chemist. They readily recognize, however, that the training received by those with degrees in analytical chemistry is not inferior but instead produces a chemist worthy of being eagerly sought after. It is paradoxical that, a t a time when analytical chemists with the doctorate are much in demand in industrial and government laboratories, there is talk of deemphasizing analytical chemistry as a curriculum subject. The controversy over the change of the content of the analytical chemistry part of the curriculum is entirely understandable. Even twenty-five years ago, i t was apparent that the analytical chemistry which was being taught in the

university was not that which was being used in industry. The very strong emphasis a t that time on gravimetric analyses when industrial laboratories were replacing gravimetric procedures whenever possible is a prime example of this. The change which has taken place in the practice of analytical chemistry must be accompanied by a corresponding change in the subject matter of the curriculum if the analytical chemist is to continue to be well-prepared for his future. As an example of the change which has occurred, the analytical chemistry course which I had as an undergraduate did not include a single experiment on colorimetric (spectrophotometric) analysis, yet probably the greatest number of the analyses which are performed currently in our Division by any single method use spectrophotometric methods. This change has, of course, Seen brought about by the fact that many spectrophotometers are now available which are designed specifically for spectrophotometric analysis. This makes a colorimetric analysis a very simple, rapid, and reasonably precise procedure, whereas previously such a technique was slow, laborious, and imprecise. The development of many other instrumental analytical techniques has followed a similar course over the same period. Instruments have been developed which are capable of performing analyses rapidly and with good precision, Immediately there has been a rush to apply the (‘new” technique, which, in many cases, a review of the literature will show that it is not a ((new” technique a t all, but that the equipment previously available for performing the analysis was inconvenient and in some cases incapable of attaining the desired precision. Thus, the great change in analytical chemistry in the past two or three decades can be attributed in large measure to the improved instrumentation which has become available during that period. Correspondingly, the training that a n analytical chemist receives must be changed from that given in the past if he expects to be able to cope with practical problems when he graduates. As to the actual content and the

REPORT

sequence of materials in the undergraduate curriculum, unfortunately I feel that I am too far removed from teaching to be able to comment in detail. It is apparent from the comments of the university professors that there are many more topics which must be covered in the present chemistry curriculum than v a s the case two or three decades ago. Obviously, if more topics are to be covered, there exist three alternatives: either some topics previously included must be omitted, the time spent on each topic must be shortened, or more courses must be required. Since there seem t o be no proposals to increase the number of required chemistry courses, only the first two alternatives seem to be feasible. To shorten the time spent on each topic, of course, has its limitations) since the corerage of each topic soon becomes so superficial that it has limited usefulness and is easily forgotten. The solution then must lie in some compromise. If more new topics are introduced, some old ones must be omitted, and probably the time spent on each topic must also be somewhat shortened, since there are some topics too basic and fundamental t o be dropped entirely. I would certainly agree with Professor Ayres that there are certain “core concepts” which can hardly be considered to be among the “easily outdated frills.” I agree again with Prof. Ayres that it mould hardly be useful to have students who can discourse glibly about all the theoretical concepts of modern chemistry, but who lack basic knowledge of the names, formulas, and properties of common chemical compounds, who cannot do simple calculations based on the stoichiometry of chemical reactions, and who have little understanding of ionic equilibria. As I have said before, the solution must lie in some sort of compromise. Some new topics must be introduced, such as a theoretical and practical understanding of some of the newer instrumental techniques, for example, A X R spectroscopy and gas chromatography, but we would hope that this would not result in the elimination of too much basic material. The way in which this compromise is effected, I am sure, will be different in different

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VOL. 38, NO. 13, DECEMBER 1966

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39 A

REPORT FOR ANALYTICAL CHEMISTS

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ANALYTICAL CHEMISTRY

schools; that is, the actual content of different courses ill vary from one school to another, but probably the overall total content of the curriculum will be similar. With such compromise courses, i t will obviously be impossible to cover all of the techniques of analysis which are in use in the modern analytical laboratory. One might ask the question then as to how the practicing analytical chemist is to become acquainted with all of these techniques. This need is being fulfilled a t least in part by the short courses on various techniques being held a t universities, at technical meetings, and being giwn by instrument makers. These courses are filling an obvious need in updating the abilities of practicing analytical chemists. With the obvious increase in material which i t seems desirable to include in a chemistry curriculum, and particularly in the analytical chemistry course, one wonders if there might be justification for considering a reritalized master’s degree t o teach some of this material with emphasis on course tvork including laboratory practice but not emphasizing a research problem and thesis as the principal goal. This is not to say that some laboratory work should not be in the nature of small research problems, but that completion of a publishable research project would not be considered the primary goal. This is not too dissimilar from a proposal I ha7.e seen described for a master’s degree for those whose primary goal is teaching and not research. I n summary, I feel that there is much new niaterial which must somehow be included in a chemistry curriculum now. Certainly there is a place for an analytical chemistry course in the present day curriculum, although it is certainly true that some of the concepts traditionally taught in analytical chemistry could equally well be taught in other courses. I think, however, that from the point of view of those seeking analytical chemists, it would be a serious error to eliminate analytical chemistry entirely. We hope that by including much new material in the chemistry curriculum that not too much of the basic principles will be pushed out.

Commenfs of W. A. KlRKLlN

The concern about education in analytical chemistry, expressed by several distinguished educators in this field in the February issue of this Journal, is shared by many. It is encouraging to know the effort being made to keep this important discipline in line with today’s needs. Going outside one’s own area to discuss matters in another is hazardous. Educational programs, however, need to take into account their purpose and the later use of the knowledge imparted. A discussion of what analytical chemists do in industry may be of interest to those planning careers in analytical chemistry and t o those who teach. The following remarks therefore will deal first with the work of analytical chemists in industry, and then only generally with education. Analytical chemistry is that area of chemistry concerned with identifying and measuring the constituents of matter, viz., the 103 presently known chemical elements and their innumerable combinations. Analytical chemistry is employed in all chemistry-inorganic, organic, and biological. It is essential for chemical synthesis, for chemical engineering and for the economical use of most chemical products. I t s specialized technology and the ever broadening need for more accurate and more precise information about the processes and materials man lives by, with, and among, demands that it be considered a discipline in itself. Reilley ( 3 ) says “Analytical chemistry is what analytical chemists do.” What does the analytical chemist do in industry? Two important areas will be discussedchemical research and chemical production. THE ANALYTICAL CHEMIST I N RESEARCH.The analytical chemist in research analyzes research products, These products may be compounds or mixtures separated from some chemical synthesis or attempted synthesis, or they may be whole reaction products. They are largely new compositions of matter, containing many unknowns. They may be solids, liquids, or gases, or combinations of them. The determination of a specific element, functional group, or chemical com-

REPORT

pound in the mixture may be called lor. The amount present may be in the p.p.m. range or less, or i t may be nearly 100 per cent. Extensive separation work by chemical or other means n i q hare to be carried out to remove interfering constituents before identifications and measurements. One compound may have t o be transformed into another for separation, identification, or measurement. Usually more than one parameter must be measured to ensure correct identification ; soinetimes complete proof of structure of a compound is necessary. Rlany such measurements can be standardized, and, where this is possible, are carried out by nonprofessional workers under the supervision of experienced chemists. Analysis of samples, however, is only a part of the analytical chemist’s work in research. He has another very important role. A. major amount of his effort is devoted to diagnosis of problems, determining analytical needs, making decisions on how best to get the desired information, evaluating and integrating the information with that of other chemists, working toward the common goal of creating or developing a new product or process, etc. To get the answers, he used x-ray, nmr, and mass spectroscopy; absorption colorimetric, spectrophotometry ; volumetric, gravimetric, and complexometric methods ; all the techniques of chromatography ; thermochemical, electrochemical, radiochemical, semimicro and micro methods; and many others. The problems may be concerned with the misbehavior of a catalyst in a reaction, the search for and identification of some impurity suspected of causing difficulty in a process, a kinetic study of a chemical reaction, or measurement of a physical constant of a compound which may involve extensive purification or even synthesis. During the writing of this paragraph, within a single hour, the author received requests for (1) critical characterization of seven different chemical compounds thought (or hoped) to be pure; 12) a quick practical method for determining fractional p.p.m., possibly p.p.b., of an exotic chemical in water; and (3) analysis of a ra-7 material for the chemical form of a

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VOL. 38, NO. 13, DECEMBER 1966

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41 A

REPORT FOR ANALYTICAL CHEMISTS

A good balance gives good results every. time. It gives you full accuracy from other instruments, too. A sleazy one can ruin experiments, waste labor, disable expensive instruments, and cost more in repairs than its purchase price. I t can never be cheap enough to be worth owning. We make good ones, For example, the GRAM Electrobalance@. It has a platinum band instead of knife edges. Better performance and reliability. No routine maintenance to remember-or forget, So rugged it has no arrestment; so stable it is used for long. term experiments: and so well built it is used in high-vacuum and corrosive atmospheres. It’s hard to. hurt. Electronic components are aerospace quality, not entertainment, and operated far below their ratings. The only active elements are silicon diodes; no transistors, no vacuum tubes, no troubles. Most instruments operate on 105-125 V. The GRAM operates on 80-135 V and holds rated performance during changes from 105-125. It has 11 sensitivities from analytical to ultramicro. 4 easily cover the same span, but 11 approach a precision of 0.01% of sample weight, instead of range. A subtle difference, but important. Its unique range switch can give 1 0 times better accuracy than the best weights, for the only real accuracy with micro samples, It comes with all normal accessories; no extra charges for the radio and heater. For specialized work we also offer 12 different sample containers, 14 different stirrups, 4 power supplies (line and battery) and a glass vacuum bottle.. Looking for ahother balance? Get a good one! U S . Patent 3,224,517

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metallic element thought to be existing in small amounts as different chemical compounds in good and bad lots of the material. Answers t o most such problems must be obtained quickly and usually call for the combined use of several analytical techniques, often with all the ingenuity that can be mustered. The analytical chemist in research needs to be aware of all ways of identifying and measuring chemical constituents. He must be able to select, develop, and prove analytical methods for new research products as they are required, and also explore and carry out research on still newer and better techniques for research’s information on the composition and chemical structure of matter. His specialized knowledge and his observations during the course of an analysis very often can be helpful to the syntheses chemist in separations and purifications for preparative purposes. The analytical chemist has to know the objectives of and be flexible to meet the ever-changing needs of research. Fundamentally, he must have the “knack” of thinking quantitatively and comprehensively ; perhaps this is one of the ways he contributes most importantly. The analytical chemist’s job in industrial research is indeed a challenging one. THE AXALYTICALCHEMIST IN PRODUCTION. Misriews are held by many in education and still even by some in industry about the role of analytical chemists in production. Too many have the idea that only routine work is involved. Industry, however, cannot afford chemists’ time and salaries for routine analytical work nor for any work that can be handled by nonprofessional people. Some comments about what the analytical chemist does in production are due. Modern chemical management has come to realize the important contributions a qualified analytical chemist can make t o the control of production processes, ensuring the quality of manufactured products (quality control), and assisting in the maintenance of and helping to make improvements in plant operations. The analytical chemist is the ‘eyes and ears’ of production, always watching for happenings or

trends that might lead to trouble. nlanufacture of an off-grade lot of product or a few hours’ breakdown of a chemical operation of any size can be very costly. Continuous attention must be given to raw material specifications and examination, surveillance of the processing, monitoring of the final product, plant wastes, safety, etc. Although this attention may be concentrated in narrow regions, the analytical chemist in production, like his counterpart in research, needs t o be broadly educated in chemistry and analytical chemistry, and in the associated areas. I n cooperation with others, he must select the analytical methods to use in production, which can range from the simplest laboratory technique to complex instrumental methods requiring costly equipment, sometimes including onstream analyzers and computers for data handling or automatic control. He must be knowledgeable about sampling and statistics and must guard costs. He must be able to work with plant management, chemical engineers, and plant operators, and he may be the intermediary between the supplier and the purchasing man or the salesman and manufacturer. He can be faced with all kinds of questions, not only about analyses but about any chemical matter, and must make judgments and recommendations for action, often on the spot. A high degree of self-sufficiency is needed. The job of an analytical chemist in production is a very responsible one. A new analytical chemist entering production work should expect to be assigned to various control duties, some of thein routine. This assignment provides opportunity to become acquainted with the chemical processes and plant operation. Following this initial training, he can look for partial or total assignment to supervision of different control analyses and tests or t o process trouble shooting o r development work where, again like the analytical chemist in research, he will be called on often t o use his analytical education in the broadest ways for solution of the problems encountered. Other responsibilities follow as ability and initiative are demonstrated. Students in their

REPORT FOR ANALYTICAL CHEMISTS

courses should be provided opportunity to learn more about production work. EDCCATIOS. Some of the work of analytical chemists in two important areas in industry has been described. Analytical chemistry is a broad subject. Proficiency in this subject requires a wide knowledge of chemistry and of science in general. Knowledge of other subjects must be acquired, too, important among which are language for effective communication (oral and written) and an understanding of our economic system. It is the earnings and profits from this system that form the sole support of all our activities and institutions. Without these profits a monolithic system under single direction could result in lost of individual freedom to select what to teach and learn and where to work. All-not just those in industry-need a good understanding of our free enterprise system. Cooperative and coordinated endeavors among all lead to the maximum benefit. As Laitinen ( 2 ) says in his editorial on “Citizenship in Science,” a good citizen or scientist properly shows loyalty to his own family or specialty in his own neighborhood or branch of science, but should demonstrate his loyalty to his country or t o his whole science when discussing problems of common interest to the whole. There are many areas of chemistry; primary among those that have come to be individually recognized are: inorganic chemistry, organic chemistry, biochemistry, physical chemistry, chemical engineering, and analytical chemistry. These divisions have evolved Tyith the necessities of time; together, they encompass the whole of chemistry. There are many subdivisions and much overlapping. They all must he considered, and our knoxledge must be reorganized and coordinated as it increases. Chemistry is a difficult science to teach and to learn. It is both abstract and concrete. Study of chemistry (starting a t the high school, even grade school level) begins with study of the elements or atoms and proceeds with how atoms are held together to form compounds. How to use chemical

laboratory equipment and handle chemicals must be learned. Let’s call this laboratory practice (not analytical chemistry, though the operations should be as quantitative as possible to develop a sense of carefulness). Mathematics, physics, and physical chemistry principles must be learned to understand x h a t is happening. The properties of the chemical elements and typical chemical compounds, and something about their origins must be learned too. (Some students will turn away from chemistry for study of mathematics, physics, etc.; they should not be discouraged, nor should their doing so be discouraging to the teacher of chemistry-because they, too, will be needed.) For those seeking careers in chemistry, we should continue t o seek ways for acquainting students with the subject matter of all the principal areas of chemistry. These are the major areas for which chemists are sought by industry, government, and I believe by educational institutions. To assist the student in selecting his major area for work, he should know the general requirements of, and the opportunities for, work in each. This broad general study then should be followed by concentrated study in the student’s area of choice t o provide him with a reasonable basis for entering industry or continuing with graduate study. The principal areas (or disciplines) of chemistry just mentioned need not be specifically defined until near the end of undergraduate study. So de-emphasizing them should minimize much of the current discussion about which of them should be taught, and where, and when, and m-hich should be required or electhe. The curriculum must, of course, include energy transitions, chemical equilibria, reaction kinetics, and the other necessary topics of chemistry, and the subject matter of all these topics must be carefully integrated and presented step-wise by qualified teachers, t o build up the student’s knowledge of chemistry. Graduate study (or extensive experience and personal study) is necessary for a comprehensive grasp of chemistry and should be pursued by those desiring careers in research or teaching in the science. Continued study See ACS Laboratory Guide for All Products/Sales Office+ Circle No. 130 on Readers’ Service Card --j

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T h e Summatic Integrator incorporates s m a l l peak accuracy, w i d e d y n a m i c r a n g e and l o w c o s t . T h e s e t h r e e desirable r e q u i r e m e n t s have n o t been available in c o m p e t i t i v e l y p r i c e d integrators until n o w . Nester/ Faust’s Sumrnatic assures y o u of the following: i A u t o m a t i c c o u n t o f each peak a t a rate w h i c h gives approximately t h e s a m e h i g h statistical reliability-regardless of peak h e i g h t up t o a maximum signal of one volt. i I P r o v e n a n d reliable voltage to frequency conversion technique t o convert t h e i n p u t s i g n a l t o a number of pulses that i s prop o r t i o n a l t o t h e area. T h i s t e c h n i q u e in c o n j u n c t i o n w i t h a n o v e l A u t o - R a n g i n g * device gives g o o d statistics o n srnaii peaks ( 1 3 % o n 1OOpv p e a k s o f 3 s e c o n d s duration) a n d a d y n a m ic r a n g e of 0 t o 1 volt DC automatically. P r e c i s i o n o n larger peaks i s a b o u t t0.7% f o r 20 m v peaks 10 s e c o n d s l o n g . Ill L o w c o s t s i n c e t h e S u n i n l a t i c ’ s A u t o - R a n g e r a l l o w s t h e u s e of a n a r r o w r a n g e 0 t o 1 niv stabilized amplifier, a n a r r o w range 0 t o 100 c p s voltage t o frequency c o n verter, a n d a f a s t m e c h a n i c a l c o u n t e r - p r i n t e r t h a t d o e s n o t req u i r e p r o v i s i o n f o r niemory. T h e A u t o - R a n g i n g circuit attenuates t h e i n p u t s i g n a l by a f a c t o r of t e n at 3 decades of s i g n a l a m p l i t u d e (1,10and100nlv)and directsthe o u t p u t f r o m t h e converter t o t h e next h i g h e r c o u n t i n g w h e e l in t h e counter-printer. A recorder o u t p u t w i t h attenuator is supplied. It operates t h r o u g h t h e A u t o - R a n g e r s o t h a t t h e pen of a 1 niv r e c o r d e r will remain o n s c a l e w i t h s i g n a l s into t h e S u m m a t i c u p t o 1 volt DC. Electronic c o n s t r u c t i o n is all solid s t a t e for l o n g life a n d reliability. W r i t e for full t e c h n i c a l literature. Nester / Faust Instrument Pro= ducts Division, 2401 Ogletown Road, Newark, Delaware. r a r e n r s o e n a in a .

REPORT FOR ANALYTICAL CHEMISTS

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after graduation will be necessary for all to keep abreast of new developments in chemistry; no scientific worker can ever quit studying. Educational institutions cannot be expected to train students in specific areas of chemistry or in specific techniques to directly fulfill industry’s needs. Industry must assunie responsibility for specific training and practice in its specific areas of work. For work in industrial analytical chemistry, however, the graduate should have, in addition to a good chemical education, a basic understanding of the principles and the potential of all the modern analytical techniques on which he can draw as needed. Coverage of these many techniques should be aided by combining diflerent topics, often taught separately, in the manner outlined by Reilley ( 3 ) viz., the interaction of electromagnetic radiation with matter: principles of rotational, vibrational, and electronic transitions; their corresponding absorption and emission spectra ; and the relationship between spectra and chemical structure. Similar coverage can be given also to the electrochemical area, and it should be possible to group the methods for chemical separations-a most important part of chemical analysis-for a reasonable understanding of them. Within these two sentences alone might be named nearly all the principal techniques of analytical chemistry, or a t least most of the important modern ones, which too often are thought of and taught as separate entities. Some practice with %7e problems” too, as mentioned by Rogers ( 4 ) is desirable. Given the basic principles, the theory, and the advanced concepts of the Iatest thinking on structure of matter in his early college work, a student interested in analytical chemistry should be able to relate and t o think in terms of the techniques of analytical chemistry. Industry needs and will continue to need competent interested people educated in analytical chemistryB.S., M.S., and Ph.D.-who can be trained to accept the responsibilities a t all levels in this vital area of its work. It is recognized that many analyses are and should be carried out directly by synthesis

chemists and others and that they, too, need to be educated in the principles of analytical chemistry. Generally, however, they cannot efficently pursue their main objectives and a t the same time be truly proficient in analytical chemistry. Their employment of a single analytical approach or selection of an analytical method or instrument just because it is known or conveniently available, “one instrunlent research,” needs t o be guarded against. Competitive industry must have accurate and as complete information about the composition of its products and materials as it can practically obtain. The opportunities for growth and advancement of an analytical chemist in industry are limited only by his ability and the amount of initiative, effort, and judgment he exercises. Rewarding careers are to be had in industrial analytical chemistry; training in this field provides a valuable basis for work in other fields as well. Kolthoff ( 1 ) writes “analytical chemists are part of the team that includes all other cheniists and engineers who are being consulted in the search for solutions t o problems which arise in producing, processing, and characterizing an industrial product.” -4s “partners in this team,” industrial and academic analytical chemists must keep alert to responsibilities of this discipline and cooperate in fulfilling them. For the education of analytical chemists, the plea is to continue searching for the best ways to bring together and coordinate all the principles and tools of analytical chemistry so as to attract, interest, and develop an analytical viewpoint in the minds of a proportionate number of the able chemistry students for analytical work-both for iiidustrial employment and for continued teaching of the subject. (1) Kolthoff, I. M., Chem. and Eng. News 146, (July 27, 1964). (2) Laitinen, H. A,, ANAL. CHEM. 38, 1105 (1966). (3) Reilley, C, N,, Ibid., 35 A (February 1966). (4) Rogers, L. B., Ibid., 53 A.

Comments of K. W. GARDINER

As an opening statement, one might say that a t the present time industry’s greatest concern with an-

REPORT

alytical chemistry is the distressing unavadabihty of profeesional analytical chermats who want to pursue an indwtzid career1 A qui& glance at the “positiom open” wtion of practically any number of recent imuen of Chemiool and En& ” e n n g New8 will provide ponvincing proof that there is a cootinuing industrial demand for people mth analytical training. l ? u r h m o ~ , the diversity of expreaKd needs and the t y p of Mustries represented belies any suggestion that employment poaeibilitien me still lwalised with the large chemical manuIacturers who have normally provided the major Bource of employment for analytical chemists. By itself, a tmimical manpmer ihortage is not mique to the analytical field, BB we all know that similar shortages in other teohnical and engineering area have been mth us for some time. However, to this writer, other techniosl weas do not seem to be plagued with the additional emotional and appw&tIy real problems of scientific identity, and even academic survival, $ha6 are now eo well associated wit21 analytical chemistry. It ia &inly unfortun& that we must haw these problems, BB analytical chemigte have been and are now enjoying a constantly improving share of the recognitions and rewards from industrial science. Yen, salsries are competitive with thase offered candidates from other branches of chemistry, and responwihifitii and growth opprhmities are equal for all1 This is not ba say that one cannot find isolated plaw where our profession does not &fer lrom the stigma of being B “&be hmction” or, at best,only a ‘‘guworting science” for the main technical endeavora of the business. Fortunately, t h e are dying sitmtiom, and such caste virtmlly extinct in modern industry. Now, fully believing thab MUE try is doing a fine job for ana chemistry, why do we hav tinuing and m t e man age? It would be easy to ise that the long-dmd tractive image of our luded to above will alasys number of people ab0 themselven to a career m chemistry. If thie limitathi is raal

R

REPORT FOR ANALYTICAL CHEMISTRY

they laughed when I sat down t the Warburg

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ANALYTICAL CHEMISTRY

and persists, then it becomes increasingly important that those who do choose analytical chemistry be giyen the very best preparation possible, as their effectiyeness will have to be just that much greater. Rather than debate the point of why promising young chemists are or are not attracted to analytical chemistry, I would like to confine my remaining remarks to some comments about certain aspects of graduate and undergraduate preparation that could, from an industrial standpoint, be a help in increasing effectiveness. First, too large a percentage of those professional analytical chemists (with the Ph.D. degree) entering industry each year are still unprepared to accept the reality that industrial analytical research, or their first on-the-job assignment, may very well be somewhat less “academic” than that experienced while doing graduate thesis Tvork. This, naturally, often leads to trouble for all parties, and then another industrial chemist is shopping around for an academic job! I think that soniewhere in his graduate program, the student should be exposed to the “facts” of industrial life. This probably could best be handled through seminars presented by able industrial spokesmen, as it goes without saying that academic people should not be involved in this sort of instruction. T o the charge that industry could improve this situation by doing better research to attract and hold these people, one can only answer that business cannot arbitrarily change its development programs and normal technical service requirements simply to fit what might be considered as attractive and satisfying work from an academic viewpoint. To me, one of the most important aspects of planning an industrial career as a technical man is to decide just as soon as possible what route-technical ladder or nianagement ladder, as they are commonly referred to-one wants to follow. This, naturally, is a very hard decision t o make when one has never been exposed to what the comparative features, pro and con, of each might be. Thus, to make my second point, exposure by the seminar route to the mechanics of getting

ahead in industry, or what business is all about, would be a most worthwhile thing. The subject matter here might include such things as the profit and loss aspects of business, where the money for research and development comes from and why spend it, the role of budgets and plans for new developments, and certain aspects of the decision making processes in a technical organization. I sincerely believe that, basically, analytical training is the best technical training one can haye as a background for top management responsibilities in a technical organization. This stems naturally from the unique requirement for a broad exposure to all areas of chemistry, as well as to a considerable amount of physics technology, that is implicit in good analytical training-a broadness usually not required in other fields of physical science. To counter the immediate argument that the above points are the things that one will learn by experience and on-the-job instruction and, therefore, should not be included in graduate level training, I would like to say that i t just does not work that way. Rarely is the technical man ever gi~7en any insight into the business operations of his company until he has actually entered the ranks of middle or top management. T o be somewhat forearmed and foreLTarned on the road up can be of inestimable value to any ambitious young man or wonian, so why not start with every advantage reasonably possible. While speaking of the intrinsic value of analytical training because of its broadness, a comment can be made about the commonly encountered high degree of technical specialization of new men entering industry. I am a firm believer that the professional analytical chemist should start his industrial career with the benefit of having had absolutely the broadest possible exposure t o the techniques, technologies and theories of analytical cheniistry. If the man is inclined toward, and is best suited for, a continuing technical role, then we (industrial management) can help him become a specialist and authority in some mutually beneficial area. A student does not have to be assigned

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narmw aspect of a profeasor's st productive (from a publicastandpoint) field of interest to ome proficient in the techniques independent research. In this the recent commenb by Pror L. B. Rogers (ANAL. Cka. 53A, 1966) are particularly ropos. From my standpoint, graduate programa are needed that will better equip candidates to solve the complex sample handling and separation problems so frequently encountered in industrial work. A b , more specific m e w of seusin& along with total bystems for detecting, identifying, and measuring components in wmplex sample streams, as normally eocountered, will always be of value. Finally, there is s continuing need for improved instmmental methods for trace analvsis of tvoical WmDlex industrial Goeeea .Leama, either gaa or liquid, snd more compatible sys, t e m for closed-loop process control. It has to be the academic research supervisor's responsibility b' develop intsmting, broad-gauge research program that will present to the graduate trainee a stimulating challenge, while at the same time they will introduce him to, and better prepare him for, the possibly more mundane aasieslments be may he given while pursuing his industrial career. Is a more cooperative relationship-and I do not mean just the supplying of money! -needed between academic and induetrial groups vis-a-vis these problems of analytical chemistry? Dr. Richard Kenyon's Editorial in Chemical and Ensinwing Newe, May 2, 1966, presents some excellent food for thought in this respect. I am nure that any number of industrial managers would be more than willing to go out of their way to help resolve those academic-versus-industrial interface problems that may be contributing to the acute shortage in analytical capshilitiea available to industry today. 90 far, my comments have been P h d y concerned with the PhD. analytical chemist who will eventually become a technical manager in industry. For the professional who wants to remain a technical staff man with little, if any, nupemisory or management respousibility, the wneept of a broad research and

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problem solving capability is, again, most valuable. To have the new graduate come to industry with a theoretical and working understanding of all the major tools of analysis would be ideal. The possibility of achieving this in a reasonable period of time ( 3 years), while also producing a thesis on original research, is not very realistic. Perhaps the greater employment of the “Compound A,’ type of thesis problem requiring the use of as many forms of analysis, both classical and instrumental, as possible, would approach the broader concept. How this broad base of capabilities and interests can be imparted t o the student is really not the industrial manager’s concern. H e is concerned, however, with the fact that the last three men he interviewed were quite positive and specific about the specialized type of work they would like, or expected, to do if they accepted employment with his particular company. To prepare a man to receive the maximum benefits from the broad capability-type of graduate program indicated above would put considerable additional strain on the current four-year undergraduate curriculum. First, it would appear that the four-year two semester, or three quarter, program is just barely adequate as it now stands. Would i t be out of the question to increase the basic bachelor’s degree program from four t o five years? For the analytical chemist in industry today, in addition to the knowledge gained in those courses normally prescribed for the bachelor’s degree, a sound working knowledge of instrument electronics and optics is practically mandatory. The ability t o improvise and innos-ate in the analytical instrument field is a plus feature that many technical managements are appreciating niore and more. It is an econoniic truism in the chemical industry that an instrumental method for a routine and repetitive test or a process measurement can more than pay for itself in the long run. I n addition, i t would be ideal if the undergraduate could approach graduate training, or industry, with a much better understanding than he now has of all the major instrumental techniques, e.g.

x-ray diffraction, emission spectrography, U.V. and I.R. spectrophotometry and gas chromatography. This is not to say that knowledge of classical wet methods is not needed, but presumably the present undergraduate curriculum is adequate in this respect. It does not seem to make very much sense to cut and cut and keep cutting useful subject matter from the undergraduate program simply because there are only four years available, and just so much will fit four years. Obviously, the scope of our knowledge in analytical chemistry is going to continue t o expand, as is the case with all other fields that are required for study, so when does one stop throwing out things to make room for the new? It seems to me that we have just about reached that limit with the four-year schedule, and consideration of expanding the time rather than compressing the subject matter might be more constructive. Finally, I think there is still substantial room for analytical chemistry to improve its image without having to engage in headbutting competitions with the other branches of the physical sciences, or by further specialization in esoteric research of little practical value conducted a t the expense of good solid instruction at the undergraduate level. For one thing, attention to the basic precepts of precision and accuracy that are the main supports of our science will do much to command respect and, a t least, could curtail the perpetuation of so-called accepted analytical text books that are inadequate for the times. Sound analytical chemistry will always be needed in industry, so it does not make much sense even t o consider its de-emphasis in, let alone its elimination from, the modern chemistry curriculum. If the university’s role is to prepare young people for a useful and gainful life, and industry is still a major outlet for achieving such goals, then those requirements of industry that are recognized as important must be considered in establishing undergraduate and graduate curricula, Academic fiat cannot eliminate the importance or value or need of analytical chemistry in industry. END